반응 #948369

반응 방정식

N4 -acetyl-N1 -hexanoylsulfanilamide

sodium hydroxide

HCl

→

N1 -hexanoylsulfanilamide

용매

water

반응 조건

후처리

1. 1
   기타After 3 hours reaction time
2. 2
   온도The solution was cooled in an ice bath
3. 3
   여과filtered
4. 4
   기타to remove sulfanilamide
5. 5
   기타to precipitate the product, N1 -hexanoylsulfanilamide, 37.9 g
6. 6
   기타This material was recrystallized from hot ethanol (75 mL)
7. 7
   기타precipitated by addition of 40 mL D.I
8. 8
   기타water to afford
9. 9
   기타recrystallized

실험 절차

N4 -acetyl-N1 -hexanoylsulfanilamide from the previous step was treated with sodium hydroxide (24.6 g) in D.I. water (200 mL) while heating to reflux. After 3 hours reaction time, the heating was stopped and the solution pH adjusted to 8 with 2N HCl. The solution was cooled in an ice bath and then filtered to remove sulfanilamide. The filtrate was acidified with aqueous HCl to pH 2 to precipitate the product, N1 -hexanoylsulfanilamide, 37.9 g. This material was recrystallized from hot ethanol (75 mL) and precipitated by addition of 40 mL D.I. water to afford recrystallized N1 -hexanoylsulfanilamide, 24.8 g (43% overall yield). H1 -NMR indicated a purity >90%.

출처